JPH01230677A - Method and apparatus for producing improved carbon black and carbon black product - Google Patents

Abstract

PURPOSE: To obtain a carbon black which provides a tire having good elasticity and wear resistance by feeding individually controlled crude streams when the carbon black is produced in a reactor by using combustion gas and crude oil.

CONSTITUTION: A reactor consisting of a combustion zone 1, a crude oil injection zone 2, a reaction zone 3, and a quenching zone 4 is prepared and injection nozzles 17 for injecting the crude oil into the crude oil injection zone 2 are provided and arranged longitudinally and laterally at intervals. Then, air and fuel 4 are introduced into the combustion zone 1 and burnt, the individually controlled carbon black crude oil streams are introduced into the injection zone 2 from the injection nozzles 17, and carbon black forming reaction is performed at individual parts in the injection zone 2 at the same time. Then the reaction is further carried on in the reaction zone 3 and quenching is performed in the quenching zone 4 to produce the carbon black.

COPYRIGHT: (C)1989,JPO

Description

DETAILED DESCRIPTION OF THE INVENTION When used for reinforcement in rubber compounds, the present invention provides
The present invention relates to a method and apparatus for producing carbon black that imparts both high elasticity and high abrasion resistance to the resulting carbon black-containing rubber compound.

In recent years, there has been a worldwide demand to improve the fuel efficiency of automobiles in order to conserve the world's limited supply of petroleum-based hydrocarbons.

Research has shown that a relatively large amount of the energy expended by a motor vehicle is used to overcome tire rolling resistance caused by hysteresis losses in the tire tread compound. Therefore, automobile manufacturers have placed stringent specifications on tires during initial installation to reduce historical rolling losses while maintaining tread wear resistance, traction, and handling characteristics.

As these standards have become increasingly required, tire suppliers are challenging their suppliers of polymers and carbon black, the two largest components in tires, by producing materials that reduce hysteresis loss in tire tread compounds. I have asked you to help.

Carbon black manufacturers have been active in efforts to develop new grades of carbon black that provide improved tread wear properties with reduced hysteresis properties while maintaining satisfactory traction and handling characteristics. Altering the balance between tread wear and hysteresis properties of carbon black has been found to be extremely difficult to achieve by conventional manufacturing methods. - In convergence, a decrease in historical value is accompanied by a decrease in tread wear resistance, and vice versa.

In a carbon black reactor with a linear flow pattern (see Figure 1), the carbon black charge feedstock is placed in a combustion zone gas stream emanating from a combustion zone located upstream of its injection point. Inside, numerous hydraulic (hydra%
lic) Injection through a spray nozzle is common practice. radially inwardly and/or outwardly, essentially at right angles to the direction of flow of the combustion hot gas stream, in order to uniformly disperse the charge feedstock into this combustion hot gas stream. It is also common to inject an atomized carbon black stock. The total flow of carbon black charge feedstock is metered as a single stream even though it is divided into multiple streams for injection into the combustion hot gas stream.

Patent-wise, the techniques described above utilizing currently used reactors do not provide carbon black with the aforementioned aspirations.

The following references are illustrative of various equipment and methods used to produce carbon black.

3.256,065 also 540,560 4,3
91.7894.360,627 4,071,49
6 4,678,8304.478.973 4,
447.401 4,383,9733.256,0
66 4,548.980 4,500,6,72
4,477.621 4.327,069 4.0
13.7604.645,657 None of these patents describe and/or teach the elements and concepts hereinafter presented as features of the present invention.

It has now been discovered that the balance between historical and trend wear values achieved by conventional manufacturing methods can be advantageously improved by modifications in the carbon black formation process.

In the present invention, the source of carbon black charge stock is split into two or more than two streams, each of which is separately metered and controlled. These separate feedstock streams are then injected through a number of hydraulic spray nozzles into discrete cross-sectional bands of the hot combustion gas stream originating from the upstream combustion chamber of the reactor. . These injection zones containing the atomized carbon black charge feedstock are separated both laterally and longitudinally in the reactor, thus producing two or more separate parallel carbon black formations. The reactions are carried out simultaneously in the reactor. By controlling the amount of feed stock injected into each of the separate injection zones, carbon black products of similar or wide range of particle sizes and/or specific surface areas can be produced simultaneously in the reactor. This method of carbon black stock injection provides a means to produce carbon black particles with a much broader size range than normally occurs when using conventional charge stock injection methods.

Those skilled in the art of carbon black production recognize that carbon black products are made up almost entirely of agglomerates in which a large number of carbon black particles are fused together to form lump and/or chain agglomerate shapes. know. These aggregates, which can vary in size and shape, are formed primarily in the reaction zone of the reactor, where a high degree of turbulence of the process gas stream containing carbon black particles occurs.

Under high temperature conditions in the reactor reaction zone, the protrusions of the particles fuse the particles into aggregates.

in that the carbon black aggregates produced by the present invention are comprised of a much wider range of particle sizes than those formed by conventional methods;
It is assumed, but should in no way be considered a limitation of the invention, that it differs from that produced by conventional methods. This change in aggregate composition is believed to play a major role in achieving the improved dynamic properties exhibited by the use of carbon black produced by the present invention.

It is therefore an object of the present invention to provide an apparatus and method by which carbon black can be produced which imparts improved dynamic properties and good tread wear in tire tread compounds used for reinforcement. .

Another object of the present invention is to produce carbon blacks having similar dynamic properties to conventionally produced carbon blacks, but with improved tread wear resistance in the rubber compounds in which they are used. The object of the present invention is to provide a device and a method for achieving this.

Yet another object of the invention is to provide new and improved carbon blacks.

Other purposes will become clear later as the explanation progresses.

The carbon black reactor shown in FIG. 1 is a modular reactor. The term "module" is used to indicate that the reactor is made up of modules or sections, each having a specific function, that are used to carry out the carbon black production process in a continuous, staged manner. are sequentially linked together to provide a means for implementing the

In longitudinal order, the reactor is divided into four sections or modules. Referring to Figure 1, section 1
is the combination of air distribution and fuel tip, part 2 is the carbon black raw material hydraulic graduate, part 3 is the reaction zone, and part 4 is the reaction quenching zone.

In operation, combustion preheated air is supplied to the carbon black reactor under sufficient pressure to overcome the pressure drop encountered in the reactor and downstream equipment. This air is in conduit 5
and into the annular space 6 between the reactor outer wall 7 and the inner combustion chamber shell 8.

This air then moves through the annular space 6 between said outer shell and inner shells 7 and 8 in the direction towards the reactor head 9.

A number of longitudinal vanes 10 are placed in the annular space 6. These vanes are rigidly attached to the internal combustion chamber shell 8 and serve three purposes. First, they impart a linear, non-rotational flow direction to the air stream. Second, they provide a heat transfer surface that transfers heat from the refractory lining 11 surrounding the combustion zone 1 through the inner shell 8 and vanes 10 to the air stream. This heat transfer partially cools the refractory lining 11 and further serves to maintain a higher flame temperature within the combustion zone 1. Third, feather 10
provides mechanical support to hold the internal combustion chamber shell 8 concentrically disposed inside the reactor shell 70.

After passing through the annular space 60 and the vane section, the combustion air passes through an air plenum chamber 12 located adjacent to the reactor head 9 and then into the combustion zone 1, located at the upstream end of the combustion zone 1. It enters through a concentric circular orifice 13.

A fuel injector 14 mounted in the reactor head is provided for injecting and dispersing hydrocarbon fuel into the combustion air stream as it passes through the orifice 13 and into the combustion chamber 1. It is being

The fuel used may be either liquid or gaseous hydrocarbon. When using liquid hydrocarbons as fuel, it is common practice to preheat the fuel to increase its evaporation rate to make ignition more rapid. Gaseous hydrocarbon fuels may be injected at or near room temperature without experiencing delayed ignition problems. It is also common practice to inject a small amount of air into the injector to cool it and prevent the metal components of the fuel pressure pump from overheating damage.

It is desirable to maintain a flame temperature as high as possible in the combustion zone 1 of the reactor while remaining within the operating temperature limits of the refractory lining in the reactor. Refractory linings of essentially pure alumina or aluminum oxide-chromium oxide composite refractories are commonly used for this application.

In the example presented herein, the air preheat temperature and fuel injection rate used are selected to provide a theoretical flame temperature of about 3500 below in combustion zone 1 in the reactor.

In addition to maintaining a high flame temperature in the reactor combustion zone 1, it is desirable to have some excess oxygen available after complete combustion of the fuel added through the fuel injector 14. This excess oxygen is depleted in the carbon black feedstock injection zone 2 of the reactor by combusting a portion of the carbon black feedstock injection in zone 2.

This additional combustion of the feedstock hydrocarbon charge not only provides supplemental heat to the carbon black formation process, but also generates a large number of combustion nuclei upon which carbon black particles are formed.

The combustion chamber in the reactor section or zone 1 is formed conically, with a maximum diameter at the upstream end of zone 1 and a continuous decrease in diameter in the downstream longitudinal direction, so that the gaseous process stream flows in the downstream direction. As you move it will continuously reduce its speed. The volumetric capacity of combustion zone I is sufficient to allow time for complete combustion of the fuel injected into the air stream through fuel injector 14. Other combustion chamber shapes may be advantageously used by those skilled in the art, however, the conical shape shown provides a homogeneous and linear flow of the combustion process hot gases into the reactor feedstock injection zone 2. provides a practical means of providing non-rotational flow.

The feedstock injection section 2 is a refractory lining zone consisting of a hot surface refractory lining 11 of the same refractory material used in the upstream fuel tank 1. A hot surface refractory lining 11 is encased in an insulating refractory material 15 to protect the shell portion 16 from excessive temperatures.

The internal shape of the raw oil injection zone 2° is divided into two parts. Its upstream part 23 is a conical continuation of the combustion zone 1 . The downstream portion 24 of section 2 is a concentric cylindrical throat of fixed diameter.

The feedstock injection zone 2 includes two or more sets of feedstock injection nozzles 17, each set of nozzles 17 being spaced apart from each other in the longitudinal and transverse directions. - Set of raw oil injection nozzles 1
7 is preferably installed in the cylindrical throat section 24 of section 20 and the set or sets of feedstock injection nozzles are installed in the upstream conical section 23 of section 2.

Each set of feed oil injection nozzles 17 are uniformly spaced around the interior periphery of the reactor cross-section and directed radially inward and generally perpendicular to the longitudinal centerline of the reactor. Consisting of a number of hydraulic or gas atomizing nozzles directed toward each other. For example 10'', 20'' from the right angle instead of right angle
, 45″, 60″, 75＠ and other suitable angles and/or spraying.
And these can be in both directions from the vertical.

When producing conventional carbon black in the conventional manner, only one set of feed oil injection nozzles is used. Which set of feedstock injection nozzles is selected is determined in part by the desired "structure" in the carbon black product being produced. Carbon black "structure" is a related term relating to the degree of carbon black particle aggregation that forms aggregates in the carbon black product produced. Carbon black “structure” is America Seein
gfor Tasting Matgrials (A
STM) Mgthads D-2414 and/or D
-3493.

Low structure carbon black products are typically produced by injecting the carbon black feedstock into section 24 of zone 2, where the maximum velocity of the process gas stream occurs. Many structures (carbon black products usually have
Produced by injecting carbon black feedstock into zone 20 section 23 where the process gas flow velocity is low. When only two sets of feed oil injection nozzles are provided in the reactor, a - set of nozzles 17 is placed in section 24 of section 2, and another set of nozzles 17 is placed inside the reactor. At a location in section 20 section 23 whose cross-sectional area is twice larger than the internal cross-sectional area of section 20 section 24,
It is customary to leave it there. It is known to those skilled in the art that further structural adjustments can be made by adding alkali metal salts into the combustion zone 1 of the reactor.

As previously mentioned, it is customary to use only one set of feed oil injection nozzles when producing conventional carbon black. FIG. 4 is a representative cross-sectional view of carbon black feedstock injection when conventional carbon black is manufactured in a conventional manner. The carbon black feedstock, preheated to near its initial boiling point, is injected radially inwardly through a number of feedstock injection nozzles 17' into the process hot gas stream generated in the combustion zone l of the reactor. . Raw material oil injection nozzle 17
' is chosen for appropriate dimensions and spray angles to effect uniform distribution of the atomized oil droplets over an internal reactor cross section as wide as is practically achievable.

This method of carbon black feedstock injection forces rapid and intimate contact between the atomized feedstock droplets and the hot combustion gas process stream flowing through zone 1 of the reactor. This means that
Carbon black results in rapid vaporization of the feedstock, thermal dissociation of hydrogen from the feedstock hydrocarbons, and pyrothermal decomposition of the hydrogen-deficient feedstock hydrocarbons into very high molecular weight pyrothermal cracking products.

Referring to FIG. 1, these reactions initiated in reactor section 2 continue at a very rapid rate as the reactant materials flow into and through reactor section 3 or zone 3. . Reaction zone 3 is a cylindrical section and has an inner diameter approximately twice the inner diameter of zone 20 section 24. This part is a hot surface refractory lining 11, enclosed inside an insulating refractory lining 18 and closed by a reactor shell 19.

As the endothermic step reaction continues in reaction zone 3 of the reactor,
The reactant mass begins to cool and condensation of the reaction products that have undergone pyrothermal decomposition begins to occur on the surface of the combustion kernels, which are generated as kings in zone 2 of the reactor. Condensation of the pyrothermal decomposition products creates extremely small spherical particles that will last as long as condensable pyrolysis products are available.
Its dimensions continue to grow.

It appears that the condensed particles that do form are initially either highly viscous liquids or semi-solid spherical particles when they are not formed. Furthermore, a continuing dehydrogenation reaction appears to occur under prevailing high temperature conditions, which transforms these particles into solid particles consisting primarily of elemental carbon.

Highly turbulent conditions occur in reaction zone 3 due to the vortex created by the rapid expansion of the reactor internal diameter between zones 2 and 3. These turbulent conditions create intense mixing of the reactant materials and promote particle collisions while they are still in their formative stages. Under these conditions,
The particles easily fuse together upon impact, creating particle agglomerates rather than individual spherical particles in the final product form.

This condensation of carbon black particles is called "structure."

Subsequent dehydrogenation of the particles occurs when the reactant material is in zone 4 of the reactor.
It continues to occur gradually as it progresses downstream into the quench zone of. The dehydrogenation reaction is finally terminated in zone 4 by cooling the reactant mass below the temperature required for dehydrogenation.

This cooling of the reactant mass is carried out by one or more quench spray nozzles 22 in the reaction quench section or quench zone 4.
This is accomplished by spraying water directly into the process stream. This water evaporates rapidly, thus cooling the process stream by absorbing heat.

The reaction quench zone 4 consists of a number of cylindrical sections lined with a temperature-resistant, spall-resistant, refractory lining and enclosed within the reactor shell 21. A number of quench spray sections 22 are provided along the longitudinal length of the zone 4, so that the reaction residence time can be adjusted by the quench section.

After cooling the process stream with water quenching, the process stream containing the entrained carbon black flows to conventional downstream equipment where subsequent heat transfer and separation of the carbon black from the remainder of the process stream is performed by conventional means. achieved. Professionals are familiar with the required downstream operations.

Process Description The process of the present invention is carried out using the carbon black reactor described above, provided that an additional carbon black feedstock control circuit is provided to control two or more than two separate carbon black feedstocks. The controlled flow is independently utilized in the operation of the process.

separately controlling the streams of two or more carbon black feedstocks and distributing these streams into separate fractions of the combustion gas thermal process stream generated in the combustion zone 1 of the reactor; thereby allowing multiple carbon black forming reactions to occur simultaneously and controlled in the same reactor, thus reducing hysteresis loss and/or increasing tread wear resistance when compounded in an automotive tire tread compound. It is possible to produce unique carbon black products. The term "automobile" refers to motorcycles, automobiles,
and all transportation vehicles such as trucks.

These carbon black products are also useful in other rubber compounding applications where low hysteresis loss, increased elasticity, and increased abrasion resistance are desired.

The operation of the reactor when using the process of the present invention, except for the process and control of the carbon black feedstock in zone 2 of the reactor, is similar to that used to produce a conventional crab pump product. Reactor operation is generally followed.

In the process of the present invention, a portion of the carbon black stock is injected and dispersed into a fraction of the combustion gas heat stream in section 23 of zone 2, and the remaining carbon black stock is injected and dispersed in section 23 of zone 20. It is injected and dispersed in the portion 24 of zone 2 in the remaining fraction of the combustion hot gas stream that is not utilized.

The relative proportions of feedstock injected in sections 23 and 24 and the relative proportions of the combustion hot gas stream employed at the carbon black feedstock injection point may be advantageously varied to produce different carbon black products.

2 and 3 are illustrations of feedstock injection in the process of the present invention, where about 50% of the hot combustion gas stream is used in zone 20 section 23 and the remaining 50% of the hot combustion gas stream is It is used in band 20 section 24. Typically, about 15 to 75% of the hot combustion gas flow is utilized within section 23 of zone 2, and the remaining 25 to 85% of the hot combustion gas flow is utilized within section 24 of zone 2. In a preferred embodiment of the process of the invention, about 25 to 5
0% is utilized within the zone 20 section and the remaining 50 to 75% of the combustion hot gas flow is utilized within the zone 20 section 24.

Similarly, the proportion of carbon black stock injected into sections 23 and 24 of zone 2 can be varied to produce carbon black products with unique properties.

Generally, about 10 to 60% of the carbon black stock may be injected into section 23 of zone 2, with the remaining 40%
90% carbon black feedstock from zone 2 part 2
Injected into 4. In a preferred embodiment of this process, 20 to 30% of the carbon black stock is injected into zone 20 section 23 and 70 to 80% of the stock is injected into zone 20 section 24.

Although it is possible to operate the process with both streams of carbon black feedstock injected at the same longitudinal location in the reactor, it is preferred that the feedstock injection locations be separated longitudinally in the reactor. , because the dynamic properties imparted by the carbon black products of the present invention ensure that the residence time of the reactant material created by the upstream feedstock injection is at least about 1 micron greater than the residence time of the downstream reactant material.
) is longer by seconds, the improvement becomes thicker.

The carbon black agglomerates formed in the reaction zone 3 of the reactor are different from the agglomerates formed in conventional processes, in that the agglomerates formed by the method of the invention are composed of particles with a broader size distribution. It is believed that they are different in that they are

It is believed that this difference in aggregate composition contributes to the improved dynamic properties of rubber formulations containing carbon black products produced by the method of the present invention. Of course, as previously stated, it is not intended to limit the invention to such assumptions other than to the features of the method, apparatus and car, bomb rack product herein described.

The following examples serve to illustrate the invention and are not intended to limit it. Parts are by weight unless otherwise specified.

A carbon black product using the method of the invention is produced in a carbon black reactor according to FIG. The dimensions of this reactor were as follows.

Combustion Zone 1 Maximum Inside Diameter 23 inches Minimum Inside Diameter 11 inches Length 72 inches Maximum Diameter 1 Section 23 11 inches Minimum Diameter, Section 23 6 inches Length, Section 23 18 inches Inside Diameter, Section 24 6 inches Length, Section 24 12 inches Reaction Reactor quench zone 4 Internal diameter 12 inches Reactor operating conditions used to produce the four products of this invention are shown in Table 1.

Operating Conditions Combustion Air Velocity, 5CFH (Standard Cubic Feet/Hour) Combustion Air Preheat Temperature Bottom Natural Gas Fuel Rate (Standard Cubic Feet/Hour) Theoretical Combustion Flame Temperature Bottom Cooling Air Velocity, 5CFH (Standard Cubic Feet/Hour) Injection of the charge stock in zone 20 - rate, lb/hr, thermal temperature, reactor internal cross-sectional area used for dispersion of the bottom stock, % Injection of charge stock in zone 11 - speed, bond/
Preheating temperature, internal cross-sectional area of reactor used for dispersing raw material oil, %-Q
TD, inch.

Distance from the discharge end of the band to the quenching water nozzle crystal
1 Experimental 140.300134,800135,100135.
30014.28012.03012.01012,1
203.5223.5103,4883,452400
450, 440 450 26.5 26.5 26.5 26.550 50
25 37.5 1.4001,540 1.3731.38150 5
0 75 62.5 Each of these experimental examples was tested for analytical values with four commercially produced conventional range carbon blacks for comparative purposes.

Each of these carbon blacks was also incorporated into rubber formulations and the properties of the resulting rubber formulations were comparatively determined.

The repulsion properties of natural rubber compositions (ASTM D3192) and styrene were measured by the pendulum repulsion method (ASTM DI054).
Butadiene synthetic rubber formulation (ASTM D3191)
Measurements were made for each of the carbon blacks. The elasticity values were compared to those obtained using industrial standard black #6 as a standard.

Each of the carbon blacks was also formulated into the following tire tread rubber formulations: Ingredients PHR Deeraden 706" 33.3 Carbon Black 70.0 Zinc Oxide 3.0 Stearic Acid 2.0 Sanolite 240"
” 2.0 Flexzo y
3- C (3) 1.0 Santokyure MOR (+J
t, 0 sulfur
2.0206.0 (1) Firest/Tire and Rubber c
o.

trademark.

(2) Trademark of Sunoil Co.

+3J Trademark of Uniroyal Chemical Co.

(4) Trademark of Monsanto Chemical Co.

Vulcanized specimens were made representative of each of the carbon blacks in the tire tread rubber formulations described above. The values of dynamic modulus, loss modulus, and loss tangent were calculated using MTS model 8.
Measurements were made on each of the specimens using the 31 Elastomer Test System.

In addition, each of the above blends was prepared in a multi-section (m
xltisection) ) used to make red Rajal-type automotive test tires and subjected these tires to road testing to determine tread wear rates for each of the formulations containing both conventional and experimental grades of carbon black. was measured.

The carbon black analysis values and rubber compound test values for each carbon black are summarized in Table 3.

The analysis values and rubber compound test values shown in Table ■ are Ame
rican 5ociety for Tasting
A/αtaria1m standardized test method or a proprietary test method used by Liteco Corporation. AST used
M test procedures are named by the appropriate A ST M test number. Descriptions of the Liteco Corporation test procedures are shown below as Tests A, B, and C.

It is known to those skilled in the art that the rolling resistance of automotive tread compounds correlates well with elasticity testing of those compounds at room temperature conditions.

Considering the test results shown in Table ■, the carbon black produced by the present invention shows that when compared to conventionally produced carbon black of similar tread wear resistance,
It has been shown that improved modulus of elasticity is provided as measured by the pendulum rebound method.

To make a comparison, N351 carbon black may be compared to Example A of the present invention. Similarly, N339 and N299
may be compared to Example B, and N234 may be compared to Examples C and D of the present invention. In all cases, the carbon blacks of the present invention have been shown to impart improved blend elasticity in both natural and synthetic rubber blend formulations.

It is also known by those skilled in the art that the rolling resistance of automobile tire tread compounds correlates well with the hysteresis loss of those compounds when tested under dynamic conditions at room temperature. Hysteresis loss can be measured directly by dynamic test equipment, and the relative history of various formulations may be derived by measuring loss tangent. (
loss modulus E'' divided by the elastic modulus E'').

Test unit Test method analysis item Iodine value III/12//g inertia C, B, (,4STM D-1510)
Nitrogen surface area M2/, , <ASTM D
-3037) NSA-iodine value -- CTAB coating area 1t/Je9.
(AST, SuZ)-3765) Average aggregate diameter nanometers (Lightco method) Tinting strength vs. ITRB percent (ASTAi D-3265) DB
P absorption number ce/1 oo gms, (A
STAi D-2414) Compressed DBp absorption number cQ/10
0gm5. CASTM D-3493) Filling density bond/cubic fee) (ASTM D-
1513) Table ■〈〈□Customary--→〉 (□This invention □〉〉66.8
89.4 104.8118.1 59.8 78.1
87.2105.470.0 92.3 107.8
119.1 80.0 88.5 108.2116.
03.2 2.9 3.0 1.0 20.2
10.4 21.0 10.673.1 90.5 1
0.24 115.4. 75.2 87.3 107
．． 7 113.5193.7 176.1 180.3
165.9 197.3186.7 173.217
5.498.6 109.2.112.8 123.1
941106.0118.0119.8121.0
120.8 123.5 124.0136.9 13
2.8139.3 133.493.5 94.4 1
06.8 104.0100.6 107.8 112
．． 2 107.922.0 22.0 22.0 21
．． 6 19,8 20.7 20,2 21.2 Test A Equipment: 1. Particle size analyzer "Nikombu 270" Source: Pacific Scientific Corp., Biatsuk/Leuco Instruments Division, 141 JIF Amen Drive Minro, O-ri, CA94025 2, Cell Day Slabter, [Artic-Model 300
J (standard with inch titanium tips) Obtained from: Altic Systems Corporation 170 Finn Fist Court Palmingdale, A'Y 11735 3. Standard laboratory model of ultrasonic bath and magnetic stirrer combination. Capacitive 50 (IJ.

Method: A sample of carbon black was dispersed in water and then placed in a Nicomp 270 analyzer to measure the aggregate average size diameter. The Nicomp machine produces dynamic light scattering (DSL) from the plow/motion of aggregates of colloidal dimensions.
(amic lighting) or photon correlation spectroscopy (photon correlation spectroscopy).
Dimensional measurements are obtained using the technique of tion 5pactro 5copy) and specialized software.

Procedure: Weigh 12 parts of carbon black into 80 parts of water in a small beaker containing a magnetic rotating rod.

Place in the ultrasonic bath for 3 minutes and remove 2 drops of solution with a dropper while still mixing. Two drops of the carbon black aqueous suspension and one drop of Triton ``Alchik Dismembrator (Di smmrnb rat o
r) Insert the J-probe tip into a beaker and apply ultrasound for 5 minutes at 80% of the indicated output. The suspension is then cooled to room temperature and transferred to a Nicomp 270. Approximately 2 million counts are taken to activate the experimental mode and ensure the stability of the output data. The Gaussian distribution/intensity combination is a current correlation model (current correlation model).
Test B Preferred for Dynamic Properties Measuring Machine: MTS Model 831 Elastomer Test System MTS
Systems Corporation, Box 24012,
Minneapolis, MN 55424 N7 Toware: MTS Basic 02.08. ((The software includes application programs supplied by MTS to perform dynamic property measurements).

Sample: The sample is a molded elastic material compound with a diameter of 2 inches/inch and a height of 1 inch.
It is an inch cylinder.

Vulcanization: Samples are vulcanized under 320°C for 20 minutes and then left for 24 hours before testing.

Test Conditions All two samples were tested at 12 Hertz.

The test temperature was below 70°C. The sample is 1 at a specific temperature.
The time has been pre-arranged. The coupons were tested under two sets of dynamic test controls.

Thirty preconditioning cycles were performed, after which the software captured the test results.

(Average load 132 psi and dynamic load 132 psi in 7() compression.

(B) Average load in compression of 132 psi and dynamic excursion of 0.0350 inch of stroke resulting in 7.0% deflection/.

Test C Method for Measuring Tread Wear Index Using the following formulation, tread sections with five linear ribs were vulcanized at 293° C. for 45 minutes in a flat mold in a laboratory press. A new P195/75R1 with eight pre-vulcanized sections, one containing control carbon black, worn out of the original tread in random order.
Applied to 4. The experimental section above is applied using a commercial pre-vulcanized tread glue cap method. Assemble four tires, each with equal parts, and drive for 5000 miles following an initial 500 mile test drive. Tire pressure is 32 psi and wheel loads are 1130 Bond. Tires in a forward X pattern
d x pattern) and measurements were taken at intervals of 1000 miles. A wear rate of 80-100 miles/mil is maintained on the control section. A regression equation is developed from the last five measurements and used to calculate the s, o o o mile loss. From these loss values, an index is calculated and the reference portion is assigned a value of 100.

Tread wear formulation Pura Dea 750" 91.7 Dera Den 706" 33.3 Carbon Black 70.0 Zinc oxide
3.0 stearic acid
2.0 Sanolite 240”
2.07 Retsukuku Zone 3-C (3)
1.0 Santo Kyoua, VOR”
1.0 sulfur
2.0 Total Weight 206.0 Loss tangent values were determined for each of the blends containing conventionally produced carbon black and carbon black produced according to the invention, and the data are presented in Table 3. Loss tangent values were measured for two Roku formulas with dynamic load injection below 70°C. The dynamic load injection frequency was controlled at 12 Hz. That is because this is the approximate rolling frequency of the test tire at a speed of 55 miles per hour.

Comparison of relative history data (loss tangent values) shows that the carbon black produced by the present invention still gives a lower history to the tread compound than the conventionally produced carbon black of equal tread wear resistance. It shows.

5 and 6 are graphical representations of loss tangent versus tread wear index comparing conventionally produced carbon black to carbon black produced by the present invention.

It is readily seen that an improved history-treadwear relationship is imparted to automotive tread tire formulations using the carbon black produced by the present invention.

[Brief explanation of the drawing]

FIG. 1 is a longitudinal cross-sectional view of a typical carbon black reactor or furnace used to carry out the method described in this invention. 2 and 3 are cross-sectional views of the carbon black reactor or furnace at points AA and BB in FIG. FIG. 4 is a cross-sectional view at point AA or BE when manufacturing carbon black by conventional procedures. FIGS. 5 and 6 are graphical representations of loss tangent versus tread wear index comparing conventionally produced carbon blacks and carbon blacks produced according to the present invention. In the figure, 1...air distribution/fuel combination zone, 2...raw material injection zone, 3...reaction zone, 4...reaction quenching zone, 12...
- Air plenum chamber and 17... injection nozzle. (Other 4 people) Foil 2 Figure I6 Cross section “AA” Figure 3 Cross section “Be” Figure 4 Carbon black charged feedstock No. 6 Treasure index procedure amendment 1.・Indication of 1986 Patent Application No. 279188 Relationship with the Carbon Black Product 3, Hi Correction Case Patent Applicant Address Name Name Liteco Corporation Procedural Amendment *<h
Patent Application No. 279188 of 1988 2, Invention Name Improved Manufacturing Method and Manufacturing Apparatus for Carbon Black, and the Carbon Black Product 3, Relationship with the Case of the Person Making the Amendment Patent Applicant Address Name Name Liteco Corporation 4, Agent Person address: Shin-Otemachi Building, 2-2-1 Hitemachi, Chiyo III-ku, Tokyo 206-ku 5, Weight of amendment order: March 1999 711 0 koku prison days) 6, Subject of amendment

Claims (1)

[Scope of Claims] 1. A method for producing carbon black in a reactor using combustion gas and a charge feedstock, in which a plurality of separately controlled streams of carbon black feedstock are injected into said reactor. into separate portions of the injection zone where carbon black particle formation begins such that multiple carbon black forming reactions are carried out substantially simultaneously in separate portions of the injection zone and into the reaction zone. said method, characterized in that said method continues in said step. 2. One of the separate carbon black feedstock injection streams and reactions is upstream of the reactor, and a second of the separate carbon black feedstock injection streams and reactions is upstream of the reactor. 2. The method of claim 1, downstream of the method. 3. The process of claim 1, wherein the residence times of the reactants in said separate parts of the reaction zone differ by at least 1/2 millisecond, and preferably by at least 1 millisecond. 4. The process of claim 2, wherein said separate injection streams of carbon black charge stock are longitudinally spaced in said reactor. 5. The method of claim 2, wherein said separate injection streams are laterally spaced within the internal cross-sectional area of said reactor. 6. The method of claim 5, wherein the upstream injection zone has a cross-sectional diameter at least about twice that of the downstream injection zone. 7. The method of claim 6, wherein the upstream injection zone and reaction zone are conical and the downstream injection zone and reaction zone are substantially cylindrical. 8. The ratio of upstream charging stock oil to downstream charging stock oil is 10:90.
8. The method of claim 7, wherein the method varies between 60:40 and 60:40. 9. A carbon black product as produced by the method of claim 1. 10. A carbon black product as produced by the method of claim 2. 11. A carbon black product as produced by the method of claim 6. 12. A rubber composition containing carbon black, characterized in that the carbon black is produced by the method according to claim 5. 13. Claim 1, wherein the rubber composition is a rubber tire composition.
2. The composition according to 2. 14. A reactor for producing carbon black using combustion gas generated in a combustion zone and charged raw material oil supplied to an injection zone, the reactor comprising the combustion zone, the injection zone, the reaction zone and 1. A reactor comprising a quench zone, the injection zone comprising a plurality of separately controlled charge feedstock injection means. 15. The reactor of claim 14, wherein said separate charge oil injection means are longitudinally spaced in said injection zone. 16. The reactor of claim 15, wherein said separate charge oil injection means are laterally spaced in an internal cross-section of said injection zone. 17. The reaction of claim 16, wherein one of said feedstock injection means is in one conical cross-section of said reactor and one is in a substantially cylindrical cross-section of said reactor. vessel.